Emile augustus babbet



E. A. BARBET.

PROCESS AND APPARATUS FOR THE CONTINUOUS TREATMENT OF FUSEL OIL.

APPLICATION FILED JUNE 10. I918.

1,389,852, Patentedsept. 6, 1921.

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K osk Iiater [C3 UNITED STATES- EMILE AUGUSTI'N BARBET, 0F PARIS, FRANCE.

rnoeEss AND APPARATUS FOR THE CONTINUOUS TREATMENT OF FUSEL-OIL.

Specification of Letters Patent.

Patented Sept. 6, 1921.

Original application filed March 6, 1914, Serial No. 822,953. Divided and this application filed June 10, 1918. Serial No. 239,314.

T 0 all whom it may concern Be it known that I, EMILE AUGUSTIN BAR- nnr, of 5 RuedelEchelle, Paris, France, manufacturer, have invented Processes and Apparatus for the Continuous Treatment of Fusel-Oil, of which the following is a full, clear, and exact description.

Fusel oils as ordinarily obtained when rectifying alcohols are turbid and malodorous, it is necessary to subject them to a treatment which renders them suitable to be put on the market.

The object of this invention is to provide a continuous process and apparatus for the treatment of fusel oil recovered in the distillation of alcohol, whereby the said oil is subjected to washing with water, the circulation of the oil through the apparatus being obtainedwithout the employment of a pump and in a very economical manner by the utilization of steam drawn from the base of the fractioning column, andthe washings be ing passed to the fractioning column for the recovery of any alcohol contained therein.

This process consists substantially:

(a) in causing these oils to be lifted into a vessel, or preferably a condenser, located at a higher level than that of the washing apparatusso as to allow of an upward flow of the oils in the latter, without using a pum (b in producing this elevation of the oils by heating the tube (in which the oils are to be raised) with steam taken from the base of the rectifying apparatus.

(0) in bringing back to the rectifying apparatus the wash water coming from the washing apparatus, this water containing the small quantity of alcohol which was present in the oils at the time they issued from the rectifying column.

The accompanying drawing shows diagrammatically a device for putting the above process into practice.

Figure 1 shows in elevation (partly in section) the whole of this apparatus and its ar-' rangement relatively to a rectifying column.

Fig. 2 is a detail view of a part of a gage tube suitable for use in connection with the apparatus.

.The washer-decanter. illustrated in Fig. 1 consists essentially of a tall, narrow cylinder 1, filled with porcelain balls or similar bodies, in order to increase the contact between the insoluble amyl alcohol and the washing water. The liquid charged with the fusel oil coming from the rectifying column A. can be measured, by the gage 2.

\Vater for washing the fusel oil can be measured by a gage 8 having an outlet in which the flow of water can readily be seen and watched. By these gages the amounts of fusel oil and watermay be adjusted as desired.

The liquid coming from the gage tube 2, and consisting of the liquid which has been taken out of the rectifying column, and consisting largely of amyl alcohol with impurities and containing a small amount of ethyl alcohol, is introduced into the decanter 1 through a pipe 4cand a perforated distributing pipe 5 which divides it into thin streams. Owing to their lesser density, these liquid streams rise toward the surface, while the wash water, which is introduced through the tube 6 and the perforated pipe 7, furnishes heavier liquid streams which descend, encountering globules of the fusel oil. Thus the washing of the oil takes place in a methodical manner, particularly owing to the innumerable changes in direction of the oil and water, due to their passage through the porcelain balls. When the globules of fusel oil reach .the upper part, above the water pipe 7, they coalesce and form a homogeneous layer of oil, which sometimes is slightly emulsified and a little turbid owing to impurities. n

The oil is finally rendered quite clear and brilliant by filtering it through a layer 8 of absorbent cotton, vegetable fibers or any other filtering substance. A similar filter may be also provided for the water passing through the gage tube 3, as illustrated at 3".

The filtered fusel oil finally overflows into the central out-flow connection 9, and thence is led to the test glass 10.

During this time, the subjacent liquid composed of the washing water and of everything which was alcoholic but not oily (including the ethyl alcohol) in the liquid extracted from the rectifier, (said liquid being composed of the water, together with everything which the said water has dissolved or taken out of the crude fusel oil),

leaves at the bottom at 11 and through the pipe 12 rises in the gage tube 13 and thence returns through the pipe 14 into the lower plates of the rectifying column A with or without previous heating.

The purified oil and the liquid free from oil issue respectively through the two outlet gage tubes 10 and 18. The gage tube 13 for the subjacent liquid is provided with a sleeve 13 (Fig. 2) sliding with a tight fit on its central tube, for controlling the discharge level and at the same time for insuring the necessary speed of output of the liquid. The tube 13 has a helical slit 13 embracing a stud 13 carried by inner tube 13 The discharge level of the gage tube 13 may be controlled in such a manner that the decanter 1 has an approximately constant layer of oil therefore there is no risk of the apparatus getting out of order or the sub jacent liquid flowing into the vessel or collector 9.

The arrangement of the decanter has given rise to a special difficulty which had to be solved, viz., it is of importance to draw off the amylic products from the rectifier in the liquid state, but then they cannot rise very high. On the other hand the subjacent liquid must be admitted to the rectifier at a suitable level; This double condition is fulfilled by the following device The fusel oils at their outlet from the rectifying column through the valve 15, descend into an inverted siphon 16 (Fig. 1) the rising arm 17 of which reaches to the top of a cooler 18 placed at a higher level than the decanter 1. In order to force the liquid to rise to this level, this rising arm 17 is surrounded by a sleeve 19 in which is supplied steam coming from the base of the rectifying column.

This steam taken at 20 is led through a pipe 21 to the sleeve 19; the water formed by the condensation of the steam flows through the pipes 22 and 23 and returns to the base of the rectifier at 24.

This steam which is supplied through 2%) and 21 and the temperature of which is from to 103 degrees, C., therefore readily boils the fusel oil which boils at about 83 to 8st degrees C. The vapor bubbles which are produced give rise to a froth and help to raise the liquid. Any retrograde movement to ward the rectifying column being impossible, a fractionation of the products cannot take place, that is to say the products which flow away from the tube 2 have a chemical composition similar to that of the liquid leaving the valve 15.

Finally, in order to permit of verifying whether the sleeve 19 is traversed through out its height by the heating steam, this sleeve is connected at its upper part by a pipe 25 with a coiled tube located. in the condenser or cooler 18; the steam which condenses in this coiled tube leaves through the tube 26.

As they issue from the washer decanter, the oils are clear and brilliant and suitable as such to be put on the market.

The present application constitutes a divi si-on of my prior application, Serial No. filed March 6, 1914,. (now Patent 1,292,676, January 28, 1919.)

1. A process for the continuous treatment of fusel oil recovered in the distillation of alcohol, which consists in causing said oils coming from the fractioning column to be levitated, by the production in a column of the oil of bubbles of vapor, to a cooling vessel at a higher level than that of the washing apparatus, so that the oil may rise through the said washing apparatus to alow level of which it is led, passing a constant stream of water into said washing apparatus at a high level thereof, withdrawing the washed fusel oil at a higher point of the washing apparatus than that of the entry of the washing water and withdrawing the washings at a lower point of the washing apparatus than that of the entry of the fusel oil.

2. A process for the continuous treatment of fusel oil recovered in the distillation of alcohol consisting inraising said oil to a cooling vessel at a higher, level than the washing apparatus by levitation by jacket-- ing the pipe through which the oil is drawn from the fractioning column with stream 100 at a suliicicnt temperature to boil said oil, leading said oil from said vessel to the base of a washing apparatus through which said oil rises in counter direction to a downward flow of washing water, and withdrawing the 105 fusel oil at the top and the washings at'the bottom of said washing apparatus.

3. A process for the continuous treatment of fusel oil recovered in the distillation of alcohol consisting in raising said oil to a cooling vessel at a higher level than a washing vessel by passing said oil through a pipe, jacketed with steam at a temperature sufiicicnt to boil said oi], passing said oil through said cooling vessel, leading said oil to the lower extremity of a washing apparatus and water to the upper extremity of said washing apparatiils and withdrawing the washed fusel oil from the upper end of said appa ratus and the washings from the lower end of said apparatus.

4. A; process for the continuous treatment of fusel oil recovered in the distillation of alcohol, consisting in raising said oil to a cooling vessel at a higher level than a washing vessel bypassing said oil through a pipe jacketed with steam taken from the base of the fractioning column, said steam being at a temperature suflicient to 'boil said oil, passing said oil through said cooling vessel, leading said oil to the lower extremity of a washing apparatus and water to the upper extremity of said washing apparatus and withdrawing the washed fusel oil from the upper end of said apparatus and the washings from the lower end of said apparatus.

5, A process for the continuous treatment of fusel oil recovered in the distillation of alcohol, consisting in raising said oil to a cooling vessel at a higher level than a washing vessel by passing said oil through a pipe jacketed with steam taken from the base of the fractioning column, said steam being at a temperature sufficient to boil said oil, passing said oil through said cooling vessel, leading said oil to the lower extremity of a washing apparatus and water to the upper extremity of said washing apparatus and withdrawing the washed fusel oil from the upper end of said apparatus and the washings from the lower end of said apparatus, said washings being returned to the rectifying column for the recovery of any alcohol contained therein.

6. A process for the continuous treatment of fusel oil recovered in the distillation of alcohol, which consists in causing said oils coming from the fractioning column to be levitated, by the production in a column of the oil of bubbles of vapor, to a cooling vessel at a higher level than that of the washing apparatus, so that the oil may rise through the said washing apparatus to a low level of which it is led, passing a constant stream of water into said washing apparatus at a high level thereof, withdrawing the washed fusel oil from the upper end of said washing apparatus and through filtering means and withdrawing the washings at the lower extremity of the washing apparatus.

7. Apparatus for purifying fusel oil comprising a rectifying column, a riser tube connected thereto at the level at which the fusel oil predominates in the liquid therein, means for heating the fusel oil in said riser tube thereby causing the fusel oil liquid to rise through said tube, an elevated condenser to which the said riser tube leads the fusel oil, a washer-decanter located at a level lower than that of said condenser, a tube connecting said condenser to the lower part of said washer-decanter, and means for causing a washing liquid to flow downwardly through the said washer-decanter.

8. Apparatus for purifying fusel oil, comprising a rectifying column, a riser tube connected thereto at the level at which the fusel oil predominates in the liquid therein, means for heating the oil in said riser tube and thereby causing the fusel oil liquid to rise through said tube, a condenser into which the said riser tube leads said fusel oil, a washer-decanter located at a level lower than that of said condenser, a tube connecting said condenser to the lower part of said washer-decanter, and means for causing a washing liquid to flow downwardly through the said washer-decanter, and a filtering device located in the upper part of said washerdecanter.

9. Apparatus for purifying fusel oil, comprising a rectifying column, a riser tube connected thereto at the level at which the fusel oil predominates in the liquid therein, means for heating the oil in said riser tube and thereby causing the fusel oil liquid to rise through said tube,- a condenser into which the said riser tube leads said fusel oil, a washer-decanter located at a level lower than that of said elevated condenser, a tube connecting said condenser to the lower part of said washer-decanter, and means for causing a washing liquid to flow downwardly through the said washer-decanter, and a pipe connection leading from the lower part of the washer-decanter, back to the rectifying column.

10. Apparatus for purifying fusel oil, comprising a rectifying column, a riser tube connected thereto at the level at which the fusel oil predominates in the liquid therein,'means for heating said oil in the riser tube by steam taken from the bottom of said rectifying column, a condenser into which the said riser tube leads said fusel oil, a washerdecanter located at a level lower than that of said elevated condenser, a tube connecting said condenser to the lower part of said washer-decanter, and means for causing a washing liquid to flow downwardly through the said washer-decanter.

11. Apparatus for purifying fusel oil, comprising a rectifying column, a riser tube connected thereto at the level at which the fusel oil predominates in the liquid therein, means for causing the fusel oil liquid to rise through said tube, an elevated condenser into which the said riser tube leads said fusel oil, a washer-decanter located at a level lower than that of said elevated condenser, a tube connecting said condenser to the lower part of said washer-decanter, gage tubes for regulating the flow of washing liquid and of fusel oil to said washer-decanter, and means for causing a washing liquid to flow downwardly through the said washer-decanter.

12. Apparatus for purifying fusel oil, comprising a rectifying column, a riser tube connected thereto at the level at which the fusel oil predominates in the liquid therein, means for causing the fusel oil liquid to rise through said tube, an elevated condenser into which the said riser tube leads said fusel oil, a washer-decanter located at a level lower than that of said elevated condenser, a tube connecting said condenser to the lower part of said washer-decanter, and means for causing a washing liquid to flow downwardly through the said washer-decanter, and gage tubes for regulating the inflow of washing liquid and of fusel oil to said washer-decanter, and for regulating the outflow of used washing liquid therefrom, adapted to maintain a predetermined height of column of washed fusel oil therein. a

18. Apparatus for purifying fusel oil, comprising a rectifying column, a riser tube connected thereto at the level at which the fusel oil predominates in the liquid therein, means for causing the fusel oil liquid to rise through said tube, an elevated condenser into which the said riser tube leads said fusel oil, a washer-decanter located at a level lower than that of said elevated condenser, a tube connecting said condenser to the lower part of said washer-decanter, and means for causing a washing-liquid to flow downwardly through the said washer-decanter, and gage tubes for regulating the inflow of washing liquid and of fusel oil to said washer-decanter, and for regulating the outflow of used washing liquid therefrom, adapted to maintain a predetermined height of column of washed fusel oil therein, and a pipe connection from the said outlet "for used washing liquid, back to said rectifying column.

14. Apparatus for purifying fusel oil, comprising a rectifying column, a riser tube connected thereto at the level at which the fuscl oil predominates in the liquid therein, means for heating this tube, an elevated condenser into which the said riser tube leads said tusel oil, a washer-decanter located at a level lower than that of said elevated condenser, said washer-decanter comprising a vertically elongated chamber, a portion thereof being filled with obstructions capable of breaking up the liquids flowing therethrough into fine streams, aninlet for fusel oil liquid near the lower part thereof, I an inlet for washing liquid located at a substantial distance above said first mentioned inlet, an outlet for washed, fusel oil located above the inlet for washing liquid, and anoutlet for used washing liquid located below the first mentioned inlet; said apparatus further comprising a tube connecting said condenser to the lower part of said washend'ecanter and means for causing a washingliquid to flow downwardly through the said washer-decanter.

The foregoing specification of my process and apparatus for the continuous separation by methodical washing of amylic oils signed by me this 21st da of May, 1918.

EMILEAUGU TIN BARBET. Witnesses v LUCIEN PAILLARD, CHAs. P. PRESSLY. 

